CN104072148B - A kind of preparation method of low cost silicon nitride honeycomb pottery - Google Patents
A kind of preparation method of low cost silicon nitride honeycomb pottery Download PDFInfo
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Abstract
The preparation method that the invention discloses a kind of low cost silicon nitride honeycomb pottery, including: step 1) preparation has the silicon nitride honeycomb base substrate of parallel channels; 2) binder removal of honeycomb body or defat; 3) calcining honeycomb body, obtains having duct inwall and stretches the silicon nitride honeycomb pottery of whisker structure. The inventive method is with silica flour for primary raw material, by controlling sintering condition, prepare matrix to be graininess, hole wall be the silicon nitride honeycomb pottery of crystal whisker-shaped, the premium properties such as this ceramic honey comb is high temperature resistant, resistance to chemical attack, it is adaptable to the filtration of multiple fluid and purification. Ceramic honey comb after using is prone to adopt multiple method to remove filtrate, reusable. The preparation method technique of the present invention is simple, and low for equipment requirements, production cost is low, and production efficiency is high, is suitable for large-scale industrial and produces.
Description
Technical field
The present invention relates to field of material technology, in particular it relates to the preparation method that one has the silicon nitride honeycomb pottery of " duct inwall stretches whisker " structure.
Background technology
Ceramic honey comb has parallel through pore structure, have osmotic pressure height, geometric jacquard patterning unit surface is big, diffusion length is short, be conducive to counting of granule to discharge and reduce the filtration advantage such as volume with gas, has a wide range of applications in the purified treatment etc. of the filtration, purification of industrial waste gas, motor-vehicle tail-gas and other life waste gas, the heat exchange of metallurgical industry and the filtration of molten metal, the toxic gas of mining industry and liquid.
For improving the work efficiency of ceramic honey comb, the hole density improving ceramic honey comb is the Main way that present stage preparation technology makes great efforts. Corning company of the U.S. adopts up-to-date ceramic honey comb product maximum 1200 through holes on the cross section of 1 square inch prepared by extruding-out process, is be currently known the method to prepare the limit in ceramic honey comb aperture. But being limited by the preparation of mould owing to the greatest problem of the method is material aperture, therefore reduced bore is very difficult further, it is difficult to preparation aperture, at the cellular material of tens micron dimensions, becomes a bottleneck problem prepared by ceramic honey comb. Namely enable the aperture reducing further ceramic honey comb and be reduced to micron dimension, its aperture reduce the increase suddenly that will cause that gas passes through resistance, thus reducing filter efficiency. That is, rely on single honeycomb texture to be difficult to solve subparticle to filter required small-bore and be maintained with air-flow this contradiction unimpeded.
Whisker is the monocrystal of a kind of high intensity beard shape of synthesis under manual control condition, and its crystal structure ratio is more complete, and internal flaw is few, and its intensity and modulus are all close to ideal crystal. Therefore, whisker frequently as reinforcing component join Metal Substrate, ceramic base and polymer-based in the effect of its activeness and quietness. Modal whisker has Si3N4、SiC、Al2O3Deng. But at present it is concentrated mainly on the preparation of whisker and in matrix activeness and quietness effect about the research of whisker, rarely have report about whisker research in other purposes. In the preparation research of whisker, it is reported that utilize hole can growth in situ whisker, such as patent CN102251284A (a kind of method preparing beta-silicon nitride whisker), and article (Ji Xiaoli, Xu Fei, power its people, Wan Weiwei, On In-situ Synthesis of Mullite Whisker enhancing silicon nitride foam ceramic, China's powder technology, 2011,17 (3): 33-36) and article (Lv Chenjing, Tian Xiushu, Han Yufang, fabricated in situ contains Al2O3Whisker Al2O3The research of/Ti-Al composite mechanism), but, former concerns is in the preparation of whisker, and rear both pay close attention to the whisker reinforced effects to matrix or foam base plate.Meanwhile, the porous body prepared by document above and the hole in parts are closed pore, it is difficult to be used for filtering.
How to overcome the dependence to aperture and unit are hole count of the legacy cellular pottery work efficiency, and then increase the pottery filtration to fine particle, and ensure the unimpeded of fluid, be current honeycomb ceramic filter and the field of purification new demand to ceramic structure.
Summary of the invention
The preparation method that the invention provides a kind of silicon nitride honeycomb pottery, comprises the following steps:
1) preparation has the honeycomb body of parallel channels and dries;
2) dried base substrate is carried out organic eliminating;
3) calcining honeycomb body, obtains body portion granule and is tightly combined, and hole inwall stretches the silicon nitride honeycomb pottery having whisker;
Described step 1) is with silica flour for raw material, and with beta-silicon nitride powder for crystal seed and diluent, after adding sintering aid, dispersant, shaping medium, deionized water mixing, preparation has the silicon nitride honeycomb base substrate of parallel channels.
Dispersant is mainly used in the colloidal formation technique such as gel injection molding and forming technology, direct coagulation casting, and the present invention is not rely on specific dispersant, as long as dispersant can so that ceramic powder suitably disperses in sauce. The example of some operable dispersants is ammonium polyacrylate, Tetramethylammonium hydroxide, ammonium citrate, ammonium polymethacrylate etc.
According to different forming methods, select corresponding shaping medium. Extrusion moulding generally selects water, polyvinyl alcohol, poly-hydroxyl ethanol acid etc. as shaping medium. Gel casting forming selects water base acrylamide polymers system to be shaping medium, and wherein monomer is acrylamide, and cross-linking agent is N, N '-methylene-bisacrylamide, and initiator is 8% ammonium persulfate solution, and catalyst is TEMED. Direct coagulation casting selects carbamide and urease to be shaping medium.
Raw material beta-silicon nitride powder involved in the present invention, Si source, C source, sintering aid powder body and the additive such as dispersant, shaping medium are common commercial powder body, its purity is commercial level, but the requirement of product purity can be adjusted basis further, also can adopt the grade reagents such as analytical pure.
The powder granularity of raw material beta-silicon nitride powder involved in the present invention, Si source, C source, sintering aid powder body and dispersant, shaping medium etc. is more little more is conducive to sintering, it is preferable that less than 2.0 μm powder body, but is not limited to this scope.
According to different forming methods, additive such as dispersant, shaping medium etc. can be different, and the solid concentration of base substrate would also vary from.
The honeycomb body in step 1) with parallel channels adopts extrusion moulding to prepare, or, in step 1), honeycomb body adopts dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopts mechanical hole building method to prepare the honeycomb body with parallel channels.
The mass percent scope of silica flour particle diameter 1000 order～3000 order described in step 1), beta-silicon nitride powder particle diameter 0.5 μm～3 μm, silica flour and beta-silicon nitride powder is in 100:0～45. 65～the 90wt% that addition is total powder body weight of silica flour and beta-silicon nitride powder. Described total powder body includes the summation of silica flour, silicon nitride powder, sintering aid and dispersant.
In the inventive method, described sintering aid is alumina powder and yttrium oxide powder, alumina powder particle diameter 0.3 μm～5.0 μm, and addition is the 4-8wt% of total powder body; Yittrium oxide particle diameter is 0.1 μm～5.0 μm, and addition is the 10-16wt% of total powder body.
Dry in step 1) is that room temperature is dried in the shade or 40～60 DEG C of drying, keeps the parallel construction in honeycomb duct.
According to different forming methods, its drying time/temperature/humidity is different, to keep base substrate indeformable for standard. Because in different forming method base substrates, content of organics is different, so it is different to get rid of organic program. In extrusion molding, dry-pressing formed prepared base substrate, content of organics is higher, depending on base substrate size, need the independent degreasing process of 1 hour to 1 day, and content of organics is relatively low in the base substrate prepared by gel casting forming and direct coagulation casting, it is easy to binder removal in rapid heating condition before sintering. This process is familiar with by those skilled in the art.
Step 2) dried base substrate is carried out organic eliminating temperature is 500～800 DEG C, the time is 0.5～3h.
Step 3) is to be placed in nitriding furnace to calcine honeycomb body, carries out nitridation reaction in flowing atmosphere or closed atmosphere, and calcining heat is 1300～1450 DEG C, and the time is 0.5～3h.
Preferred calcination temperature is 1450 DEG C, it is preferable that the time is 3h.
Described nitriding furnace is the tube furnace of Si-Mo rod calandria. Avoid using hot pressing furnace or the carbon shirt-circuiting furnace of graphite heating body, it is prevented that carbon pollutes.
Described atmosphere is the one in following gas or mixing gas: nitrogen, ammonia, nitrogen and hydrogen, nitrogen and argon.
Preferably, in above-mentioned mixing gas, nitrogen and hydrogen volume are 9～1:1 than for 95:5, nitrogen and argon volume ratio.
Present invention also offers the preparation-obtained silicon nitride honeycomb pottery of above-mentioned preparation method.
The present invention proposes on the framework of ceramic honey comb base substrate, utilize the principle of hole growth whisker, prepare the whisker stretched in silicon nitride honeycomb this new structure silicon nitride honeycomb ceramic channel walls of pottery of " whisker intert parallel channels " new structure that hole wall is whisker and can effectively carry out the filtration of fine particle, and its original basic honeycomb parallel via holes structure in turn ensure that the smoothness of fluid. Breach the dependence to pottery unit are hole count of the legacy cellular ceramic filter efficiency.
The production technology of the present invention is simple, low for equipment requirements, convenient operation and control, and production efficiency is high, is suitable for large-scale industrial and produces. The ceramic honey comb prepared by the method for the present invention is silicon nitride material, there is the premium properties such as high temperature resistant, resistance to chemical attack, filtration and purification suitable in multiple fluid, the filtration, purification of fine particle, waste gas that various industrial process produces, its other life waste gas of motor-vehicle tail-gas in air, it may also be used for the purified treatment etc. of the tabular adsorbate of analysis chromatographic column, the filtration to the heat exchange of metallurgical industry and molten metal, the toxic gas to mining industry and liquid. Scanning electron microscope (SEM) shows that the ceramic honey comb body portion granule of the present invention is tightly combined, and honeycomb hole inwall grows into whisker, forms parallel channels. This structure makes the ceramic honey comb of the present invention can pass through the smoothness of straight channels maintenance fluid in use, and the whisker that passing hole channel inwall stretches filters further, purifies fluid. The present invention adopts silica flour to replace beta-silicon nitride powder, not only cost of material is substantially reduced, and sintering temperature is also reduced to the silica flour reaction-sintered temperature of maximum 1400 DEG C by the silicon nitride sintering temperature of at least 1650 DEG C, and whole process costs is greatly reduced, save the energy and production cost, be beneficial to industrialization.
Accompanying drawing explanation
Fig. 1 is the silicon nitride ceramics SEM photograph of concrete " duct inwall stretches whisker " that embodiment 1 prepares.
Fig. 2 is the silicon nitride ceramics XRD figure of concrete " duct inwall stretches whisker " that embodiment 1 prepares.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention. Without departing from the spirit and substance of the case in the present invention, the amendment that the inventive method, step or condition are made or replacement, belong to the scope of the present invention.
If not specializing, chemical raw material used in embodiment is conventional commercial raw material, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Silicon nitride honeycomb pottery and performance thereof are prepared in embodiment 1 extrusion molding
Taking the silica flour that 200g particle diameter is 3000 orders, 5g particle diameter is the aluminium oxide of 1.0 μm and yittrium oxide that 15g particle diameter is 2.0 μm, and mix homogeneously obtains mixture of powders. Water, polyvinyl alcohol and poly-hydroxyl ethanol acid are pressed the weight ratio mixing of 70:10:20, stirring prepares homogeneous solution, solution is mixed according to the weight ratio of 100:70 with above-mentioned powder mixture, fully mixing 0.75 hour of room temperature in mixing roll (BL-6175-B) at normal temperatures and pressures, under normal temperature and pressure old 3 hours, obtain pug. Pug is crossed 60 mesh sieves be filtered purifying, honeycomb biscuit is extruded by honeycomb ceramic extruding machine (BL-6177), 40 DEG C dry 6 hours, dried sample is at 600 DEG C of binder removal organics removal 2h, then the honeycomb biscuit after binder removal is put in tube furnace (GSL-1600X), it is warming up to 1350 DEG C with 10 DEG C/min, under blanket of nitrogen, is incubated 2.5 hours, be there is the silicon nitride honeycomb pottery of " duct inwall stretches whisker " structure. Its SEM photograph is shown in Fig. 1, and XRD figure is shown in Fig. 2. SEM photograph shows that the silicon nitride honeycomb ceramic matrix partial particulate that the present embodiment prepares is tightly combined, and honeycomb hole inwall grows into whisker, forms parallel channels.
This ceramic honey comb aperture is 0.5mm, and the porosity is 60%. Detecting according to the GB/T1964 method specified, obtaining horizontal comprcssive strength is 5MPa, axial compression strength 15MPa. After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good. After testing, the excellent specific properties such as the silicon nitride honeycomb pottery of preparation has osmotic pressure height, geometric jacquard patterning unit surface is big, diffusion length is short, be conducive to counting of granule to discharge and reduce filtration volume with gas, the smoothness of fluid. And adopt silica flour to replace silicon nitride to be prepared pottery, with low cost.
Embodiment 2 gel casting forming prepares silicon nitride honeycomb pottery and performance thereof
By monomeric acrylamide and cross-linking agent N, N '-methylene-bisacrylamide is dissolved in water, monomer concentration is 15wt%, crosslinker concentration is 0.5wt%, form monomer premixed liquid, 100ml monomer premixed liquid adds the silicon powder 200g that particle diameter is 3000 orders, add the beta-silicon nitride powder 10g of particle diameter 0.5 μm, add 1 μm of alumina powder 5.75g of sintering aid particle diameter and 1 μm of yttrium oxide powder 17.25g of particle diameter, dispersant is ammonium citrate 2g, stirring obtains the ceramic size that solid concentration is about 40%, above-mentioned slurry adds catalyst n, N, N ', N '-tetramethylethylenediamine 25 μ l, then stir, add initiator 8% ammonium persulfate solution 50 μ l, mould is injected at once after stirring, and self-control Multi needle is become punch die (syringe needle φ=2mm, 4 hole/square centimeters) insert in slurry, it is the demoulding after gel until slurry, obtain the wet base of honeycomb. wet base is put into 50 DEG C of baking oven dry 24 hours, dry base substrate is put in tube furnace (GSL-1600X), it is warming up to 1350 DEG C with 10 DEG C/min of speed, in temperature-rise period, Organic substance completes to get rid of, under nitrogen and 5% hydrogen mixed gas atmosphere, 1350 DEG C are incubated 3 hours, are had the silicon nitride honeycomb pottery of " duct inwall stretches whisker " structure.The SEM photograph of the silicon nitride honeycomb pottery that the present embodiment prepares is similar with the silicon nitride honeycomb pottery that embodiment 1 prepares with XRD figure.
This ceramic honey comb aperture is 0.1mm, and the porosity is 65%. Detecting according to the GB/T1964 method specified, obtaining horizontal comprcssive strength is 7MPa, axial compression strength 15MPa. After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good. After testing, the excellent specific properties such as the silicon nitride honeycomb pottery of preparation has osmotic pressure height, geometric jacquard patterning unit surface is big, diffusion length is short, be conducive to counting of granule to discharge and reduce filtration volume with gas, the smoothness of fluid. And adopt silica flour to replace silicon nitride to be prepared pottery, with low cost.
Embodiment 3 is dry-pressing formed prepares silicon nitride honeycomb pottery and performance thereof
Silica flour by 200g particle diameter 1000 order, 3 μm of beta-silicon nitride powders of 20g particle diameter, 1 μm of sintering aid alumina powder of 5g particle diameter and 2 μm of yttrium oxide powder mix homogeneously of 15g particle diameter, add ethanol and abrading-ball wet grinding 24 hours, after drying and screening, add using material 5wt% paraffin after sieving as forming agent, punching block is pressed into strip sample (long 10cm, wide 5cm, high 5cm), pressure is 120MPa, it is then pressed into self-control Multi needle and becomes punch die (syringe needle φ=2mm, 4 hole/square centimeters) and extract, prepare honeycomb body, this honeycomb body is put into and draft glue discharging furnace is warming up to 800 DEG C and is incubated dewaxing in 3 hours, dry base substrate is put in tube furnace (GSL-1600X), it is warming up to 1400 DEG C with 10 DEG C/min of speed, it is incubated 1 hour under ammonia atmosphere, be there is the silicon nitride honeycomb pottery of " duct inwall stretches whisker " structure. the SEM photograph of the silicon nitride honeycomb pottery that the present embodiment prepares is similar with the silicon nitride honeycomb pottery that embodiment 1 prepares with XRD figure.
This ceramic honey comb aperture is 0.1mm, and the porosity is 60%. Detecting according to the GB/T1964 method specified, obtaining horizontal comprcssive strength is 5MPa, axial compression strength 12MPa. After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good. After testing, the excellent specific properties such as the silicon nitride honeycomb pottery of preparation has osmotic pressure height, geometric jacquard patterning unit surface is big, diffusion length is short, be conducive to counting of granule to discharge and reduce filtration volume with gas, the smoothness of fluid. And adopt silica flour to replace silicon nitride to be prepared pottery, with low cost.
Embodiment 4 direct coagulation casting prepares silicon nitride honeycomb pottery and performance thereof
By the silica flour of 300g particle diameter 3000 order, 3 μm of beta-silicon nitride powders of 20g particle diameter, 2 μm of sintering aid alumina powders of 8.5g particle diameter and 5 μm of yttrium oxide powder mix homogeneously of 25g particle diameter, add 100ml deionized water to be sufficiently stirred for, slurry is cooled to about 5 DEG C, add analytically pure carbamide 1g and urease 20unit/mg, it is stirred well to uniformly, slurry is warming up to 25 DEG C, self-control Multi needle is become punch die (syringe needle φ=2mm, 4 hole/square centimeters) put in slurry, static 1 hour, slurry curing, takes out Multi needle and becomes punch die, prepare silicon nitride honeycomb base substrate. Base substrate is put into 40 DEG C of baking oven dry 12 hours, dry base substrate is put in tube furnace (GSL-1600X), it is warming up to 1400 DEG C with 10 DEG C/min of speed, in temperature-rise period, Organic substance completes to get rid of, nitrogen and lower 1400 DEG C of 5% argon mixed atmosphere are incubated 2 hours, are had the silicon nitride honeycomb pottery of " duct inwall stretches whisker " structure.The SEM photograph of the silicon nitride honeycomb pottery that the present embodiment prepares is similar with the silicon nitride honeycomb pottery that embodiment 1 prepares with XRD figure.
This ceramic honey comb aperture is 0.1mm, and the porosity is 66%. Detecting according to the GB/T1964 method specified, obtaining horizontal comprcssive strength is 5MPa, axial compression strength 13MPa. After placing 24 hours again after ceramic honey comb is boiled 0.5 hour with 10% salpeter solution, solution is water white transparency, and resist chemical performance is good. After testing, the excellent specific properties such as the silicon nitride honeycomb pottery of preparation has osmotic pressure height, geometric jacquard patterning unit surface is big, diffusion length is short, be conducive to counting of granule to discharge and reduce filtration volume with gas, the smoothness of fluid. And adopt silica flour to replace silicon nitride to be prepared pottery, with low cost.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the technology of the present invention principle; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of the silicon nitride honeycomb pottery of a low cost, it is characterised in that described method comprises the following steps:
1) preparation has the honeycomb body of parallel channels and dries;
2) dried base substrate is carried out organic eliminating;
3) calcining honeycomb body, obtains body portion granule and is tightly combined, and hole inwall stretches the silicon nitride honeycomb pottery having whisker;
Described step 1) it is with silica flour for raw material, with beta-silicon nitride powder for crystal seed and diluent, after adding sintering aid, dispersant, shaping medium, deionized water mixing, preparation has the silicon nitride honeycomb base substrate of parallel channels;
Wherein, the 65～90wt% that addition is total powder body weight of silica flour and beta-silicon nitride powder;
Described total powder body is the summation of silica flour, silicon nitride powder, sintering aid and dispersant;
Described sintering aid is alumina powder and yttrium oxide powder;
Step 3) it is be placed in nitriding furnace to calcine honeycomb body, in flowing atmosphere or closed atmosphere, carry out nitridation reaction, calcining heat is 1300～1150 DEG C, and the time is 0.5～3h.
2. preparation method as claimed in claim 1, it is characterized in that, step 1) in have parallel channels honeycomb body adopt extrusion moulding prepare, or, step 1) in honeycomb body adopt dry pressing, gel casting forming method or direct coagulation casting method first to prepare biscuit, then adopt mechanical hole building method to prepare the honeycomb body with parallel channels.
3. preparation method as claimed in claim 1, it is characterised in that step 1) described silica flour particle diameter 1000 order～3000 order, beta-silicon nitride powder particle diameter 0.5 μm～3 μm.
4. preparation method as claimed in claim 1, it is characterised in that described sintering aid is alumina powder and yttrium oxide powder, alumina powder particle diameter 0.3 μm～5.0 μm, and addition is the 4-8wt% of total powder body; Yittrium oxide particle diameter is 0.1 μm～5.0 μm, and addition is the 10-16wt% of total powder body.
5. preparation method as claimed in claim 1, it is characterised in that step 1) in dry be that room temperature is dried in the shade or 10～60 DEG C of drying, the parallel construction in maintenance honeycomb duct.
6. preparation method as claimed in claim 1, it is characterised in that step 2) dried base substrate is carried out organic eliminating temperature is 500～800 DEG C, the time is 0.5～3h.
7. preparation method as claimed in claim 1, it is characterised in that described nitriding furnace is the tube furnace of Si-Mo rod calandria.
8. preparation method as claimed in claim 1, it is characterised in that described atmosphere is the one in following gas or mixing gas: nitrogen, ammonia, nitrogen and hydrogen, nitrogen and argon.
9. the silicon nitride honeycomb pottery that the arbitrary described method of claim 1～8 prepares.
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| CN105837223A (en) * | 2016-05-04 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for synthesizing aluminum nitride power |
| CN106699227B (en) * | 2017-01-13 | 2019-05-24 | 武汉科技大学 | A kind of nano wire self-reinforcing porous silicon nitride ceramic and preparation method thereof |
| CN112661519A (en) * | 2021-01-28 | 2021-04-16 | 威海圆环先进陶瓷股份有限公司 | Production technology of silicon nitride ceramic pile |
| CN114853500B (en) * | 2022-04-29 | 2023-04-07 | 中国科学院上海硅酸盐研究所 | Silicon nitride and silicon carbide combined complex phase ceramic and preparation method and application thereof |
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